CN101278184B - Shear measuring method and its device - Google Patents
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- 239000007788 liquid Substances 0.000 claims description 14
- 239000010409 thin film Substances 0.000 claims description 7
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- 238000005461 lubrication Methods 0.000 description 10
- 239000010445 mica Substances 0.000 description 7
- 229910052618 mica group Inorganic materials 0.000 description 7
- QPYKYLANDNYEIF-UHFFFAOYSA-N 1-hexyl-4-phenylcyclohexa-2,4-diene-1-carbonitrile Chemical group C1=CC(CCCCCC)(C#N)CC=C1C1=CC=CC=C1 QPYKYLANDNYEIF-UHFFFAOYSA-N 0.000 description 6
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- 230000000704 physical effect Effects 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
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- 229910052594 sapphire Inorganic materials 0.000 description 1
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N19/00—Investigating materials by mechanical methods
- G01N19/04—Measuring adhesive force between materials, e.g. of sealing tape, of coating
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
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Abstract
本发明提供一种共振切变测定方法,其在试样的剪切响应的测定中,对试样的单侧表面的振动的衰减曲线进行傅立叶变换,来取得共振切变曲线,从而可进行其简便的短时间测定。在共振切变测定方法中,将输入信号Uin输入到共振切变测定单元的水平驱动部,使用位移计对该共振切变测定单元中的固体表面中夹入的试样的单侧表面的振动进行检测来作为输出信号Uout,与所述输入信号Uin一起,将所述输出信号Uout输入到共振切变计量装置,将所述共振切变测定单元的固体表面中夹入的试样的剪切响应与膜厚的变化一起进行计量,其中,使用傅立叶变换部(5B)对所述试样的单侧表面的振动的衰减曲线进行傅立叶变换,来取得共振切变曲线。另外,提供一种双路型切变应力测定装置,其使用可对不透明基板间的距离进行测定的双路法可进行精密的切变应力测定。
The present invention provides a method for measuring the resonance shear. In the measurement of the shear response of the sample, Fourier transform is performed on the vibration attenuation curve of the surface of one side of the sample to obtain the resonance shear curve, so that the resonance shear curve can be obtained. Simple short-time measurement. In the resonance shear measurement method, the input signal U in is input to the horizontal driving part of the resonance shear measurement unit, and the displacement of one side surface of the sample sandwiched by the solid surface in the resonance shear measurement unit is measured using a displacement meter. Vibration is detected as an output signal U out , together with the input signal U in , the output signal U out is input to the resonance shear measurement device, and the test sample sandwiched in the solid surface of the resonance shear measurement unit is The shear response of the sample was measured together with the change of the film thickness, and the resonance shear curve was obtained by performing Fourier transform on the vibration attenuation curve of one side surface of the sample using the Fourier transform unit (5B). In addition, there is provided a dual-path shear stress measurement device capable of precise shear stress measurement using a dual-path method capable of measuring the distance between opaque substrates.
Description
技术领域 technical field
本发明涉及不论是透明或不透明中的哪一个都可对2个固体表面间或其间的薄膜进行期望的测定的切变测定方法及其装置,更具体而言,特别涉及(1)进行厚度容易地变化的膜和挥发性高的液体膜等的测定的迅速、简便、通用且精密的共振切变测定方法及其装置、(2)通过基于双路型干涉法的表面间距离计量,以纳米等级改变二个固体表面的间隔并对其间夹入的液体薄膜·液晶薄膜·高分子吸附层等之间的切变应力进行测定的测定方法及其装置。The present invention relates to a shear measurement method and its device capable of performing desired measurement of a thin film between two solid surfaces or between two solid surfaces regardless of whether it is transparent or opaque, and more specifically relates to (1) measuring the thickness easily Rapid, simple, versatile and precise resonance shear measurement method and its device for the measurement of changing films and highly volatile liquid films, etc. A measuring method and device thereof for measuring the shear stress between a liquid film, a liquid crystal film, a polymer adsorption layer and the like sandwiched therebetween while changing the distance between two solid surfaces.
背景技术 Background technique
(1)首先第1(1)First of all 1st
将固体表面中夹入的试样(液体·液晶等)的剪切响应与纳米等级的膜厚的变化一起得知的技术,在固体表面间的摩擦·润滑以及液体·液晶分子的定向·结构化的理解以及控制中是重要的。在对试样的剪切响应进行测定的共振切变测定中,使单侧表面沿着水平方向振动来对试样赋予剪切,并在共振频率附近对该响应进行监视。将该剪切响应作为频率的函数而绘制出的结果为共振曲线。共振频率以及共振峰值的高度对固体表面间的试样的物性敏感并对来自测定装置外部的振动噪声也较强。Technology to know the shear response of a sample (liquid, liquid crystal, etc.) sandwiched between solid surfaces together with changes in film thickness at the nanometer level, friction and lubrication between solid surfaces, and orientation and structure of liquid and liquid crystal molecules It is important in the understanding and control of culture. In the resonance shear measurement for measuring the shear response of a sample, shear is applied to the sample by vibrating one side surface in the horizontal direction, and the response is monitored near the resonance frequency. The result of plotting this shear response as a function of frequency is the resonance curve. The resonance frequency and the height of the resonance peak are sensitive to the physical properties of the sample between the solid surfaces and are also strong against vibration noise from outside the measurement device.
以往,为了精密地得知固体表面中夹入的试样的剪切响应,进行如下的动作:在共振频率附近一边改变频率一边对试样的剪切响应进行测定,由此取得对频率进行绘制出的共振切变曲线。例如在下述非专利文献1中公开有这样的技术。Conventionally, in order to accurately know the shear response of a sample sandwiched by a solid surface, the following operation was performed: the shear response of the sample was measured while changing the frequency around the resonance frequency, and the frequency plotted The resulting resonance shear curve. Such a technique is disclosed in, for example, Non-Patent Document 1 below.
另外,已提出作为基于本申请发明者的提案的精密切变应力测定装置(下述专利文献1)。In addition, a precision strain stress measuring device based on the proposal of the inventors of the present application has been proposed (Patent Document 1 below).
专利文献1:专利第3032152号公报Patent Document 1: Patent No. 3032152
非专利文献1:液晶 第6卷 第1号 p34-41 2002Non-Patent Document 1: Liquid Crystals Volume 6 No. 1 p34-41 2002
(2)第2,本申请发明者已经提出可高精度地对纳米等级的微小空间中的流变学(rheology)游动进行测定的精密切变应力测定装置(参照下述专利文献2)。(2) Second, the inventors of the present application have proposed a precision strain-stress measuring device capable of measuring rheological movement in nanometer-order minute spaces with high precision (see Patent Document 2 below).
另外,已提出即使是光无法透过的试样也可以以高精度对试样间的表面力进行测定的表面力测定装置及其方法(参照下述专利文献3)。In addition, a surface force measurement device and a method thereof have been proposed that can measure the surface force between samples with high precision even if the sample is opaque to light (see Patent Document 3 below).
专利文献2:专利第3032152号公报Patent Document 2: Patent No. 3032152
专利文献3:特开2001-108603号公报Patent Document 3: JP-A-2001-108603
但是,在上述(1)的以往技术中,由于一边改变振动频率一边在共振频率附近对试样的剪切响应进行测定,所以需要长时间将试样的膜厚保持为恒定,存在难以进行厚度容易地变化的膜和挥发性高的液体薄膜的测定的问题。However, in the conventional technique of (1) above, since the shear response of the sample is measured near the resonance frequency while changing the vibration frequency, it is necessary to keep the film thickness of the sample constant for a long time, and it is difficult to measure the thickness. Determination of easily changing films and thin films of highly volatile liquids.
另外,作为上述(2)的以往的技术,为了一边以0.1纳米的分辨率对表面间距离进行测定一边对表面中夹入的试样的粘弹性以及摩擦·润滑特性进行测定,采用将基于使用等色序干涉条纹(FECO)的光干涉法的表面间距离测定和切变共振测定装置进行组合的方法。该方法由于使用透过表面的光,所以基板以及基板表面中夹入的试样限于光透过性的试样。特别,基板在实用上大致限于云母,即使在试验中也仅将蓝宝石或玻璃的薄片(厚度为2μm左右)使用为基板。In addition, as the conventional technology of (2) above, in order to measure the viscoelasticity and friction and lubrication characteristics of the sample sandwiched between the surfaces while measuring the distance between the surfaces with a resolution of 0.1 nm, the A method that combines the distance measurement between surfaces by the optical interferometry of equichromatic interference fringes (FECO) and a shear resonance measurement device. Since this method uses light transmitted through the surface, the substrate and the sample sandwiched between the substrate surface are limited to light-transmitting samples. In particular, practically, the substrate is generally limited to mica, and only a thin piece of sapphire or glass (about 2 μm in thickness) was used as the substrate even in the test.
另外,双路型表面力测定装置(上述专利文献3)是测定对上下表面作用的力的装置,无法进行切变测定。In addition, the two-way surface force measuring device (the above-mentioned Patent Document 3) is a device for measuring the force acting on the upper and lower surfaces, and cannot perform shear measurement.
发明内容 Contents of the invention
本发明的目的在于提供一种不论试样是透明或者不透明中的哪一个都可进行期望的测定的切变测定方法及其装置。An object of the present invention is to provide a shear measurement method and an apparatus thereof that can perform desired measurement regardless of whether a sample is transparent or opaque.
在更具体地叙述时,In more specific terms,
鉴于上述状况,本发明的第1目的在于提供一种共振切变测定方法,其中,在试样的剪切响应的测定中,对试样的单侧表面的振动的衰减曲线进行傅立叶变换,取得共振切变曲线,从而可进行其简便的短时间测定。In view of the above situation, the first object of the present invention is to provide a resonance shear measurement method, wherein, in the measurement of the shear response of the sample, Fourier transform is performed on the attenuation curve of the vibration of one side surface of the sample to obtain Resonance shear curve, so that it can be easily measured in a short time.
另外,鉴于上述状况,本发明的第2目的在于提供一种双路型切变应力测定方法及其装置,其中,使用在基板或试样为不透明的情况下可对基板间的距离进行测定的双路法,可进行精密的切变应力测定。In addition, in view of the above situation, the second object of the present invention is to provide a two-way type shear stress measurement method and its device, wherein the distance between the substrates can be measured when the substrate or the sample is opaque. Two-way method for precise shear stress measurement.
本申请发明为了达成上述目的,In order to achieve the above object, the invention of the present application,
(1)在共掁切变测定方法中,将输入信号Uin输入到共振切变测定单元的水平驱动部,针对该共振切变测定单元中的固体表面中所夹入的试样,使用位移计对其单侧表面的振动进行检测来作为输出信号Uout,并与所述输入信号Uin一起,将所述输出信号Uout输入到共振切变计量装置,将所述共振切变测定单元的固体表面中所夹入的试样的剪切响应与膜厚的变化一起进行计量,其特征在于,对所述试样的单侧表面的振动的衰减曲线进行傅立叶变换,来取得共振切变曲线。(1) In the resonant shear measurement method, the input signal U in is input to the horizontal driving part of the resonance shear measurement unit, and the displacement The vibration of the surface on one side of the meter is detected as the output signal U out , and together with the input signal U in , the output signal U out is input to the resonance shear measurement device, and the resonance shear measurement unit The shear response of the sample clamped in the solid surface of the sample is measured together with the change of the film thickness, and it is characterized in that the attenuation curve of the vibration of the one-sided surface of the sample is subjected to Fourier transform to obtain the resonance shear curve.
(2)在共振切变测定方法中,将输入信号Uin输入到共振切变测定单元的水平驱动部,在固体表面间不夹入试样而将固体表面本身作为试样,使用位移计对该共振切变测定单元中的试样的单侧表面的振动进行检测来作为输出信号Uout,并与所述输入信号Uin一起,将所述输出信号Uout输入到共振切变计量装置,将所述共振切变测定单元的所述试样的剪切响应与膜厚的变化一起进行计量,其特征在于,对所述试样的单侧表面的振动的衰减曲线进行傅立叶变换,来取得共振切变曲线。(2) In the resonance shear measurement method, the input signal U in is input to the horizontal driving part of the resonance shear measurement unit, and the solid surface itself is used as the sample without sandwiching the sample between the solid surfaces, and the displacement gauge is used to measure the The vibration of one side surface of the sample in the resonance shear measurement unit is detected as an output signal U out , and together with the input signal U in , the output signal U out is input to the resonance shear measurement device, The shear response of the sample of the resonance shear measurement unit is measured together with the change of the film thickness, and it is characterized in that the attenuation curve of the vibration of the surface of one side of the sample is subjected to Fourier transform to obtain Resonance shear curve.
(3)在上述(1)记载的共振切变测定方法中,其特征在于,所述试样为薄膜。(3) In the resonance shear measurement method described in (1) above, the sample is a thin film.
(4)在上述(1)记载的共振切变测定方法中,其特征在于,所述试样为液体。(4) In the resonance shear measurement method described in (1) above, the sample is a liquid.
(5)在上述(1)记载的共振切变测定方法中,其特征在于,所述试样为液晶。(5) In the resonance shear measurement method described in (1) above, the sample is a liquid crystal.
(6)在上述(1)记载的共振切变测定方法中,其特征在于,所述试样为纳米尺寸的厚度。(6) In the resonance shear measurement method described in (1) above, the sample has a nanometer-sized thickness.
(7)在上述(1)或(2)记载的共振切变测定方法中,其特征在于,通过吸附或化学修饰法对所述试样的表面进行修饰。(7) In the resonance shear measurement method described in (1) or (2) above, the surface of the sample is modified by adsorption or chemical modification.
(8)在上述(1)或(2)记载的共振切变测定方法中,其特征在于,所述共振切变曲线为所述试样的剪切响应的频率特性。(8) In the resonance shear measurement method described in (1) or (2) above, the resonance shear curve is a frequency characteristic of the shear response of the sample.
(9)一种共振切变测定装置,其特征在于,该共振切变测定装置具有:波形发生器;电源,与该波形发生器连接;共振切变测定单元,与该电源连接且被输入输入信号Uin;位移计,与该共振切变测定单元连接;共振切变测定装置,与该位移计以及所述电源连接且被输入输出信号Uout以及输入信号Uin,该共振切变测定装置具有计时部、与该计时部和所述位移计连接的傅立叶变换部、与该傅立叶变换部连接的振幅谱生成部、振幅(Uout/Uin)的标准部、以及共振切变曲线制成部;以及计算机,与所述波形发生器和共振切变测定装置连接。(9) A resonance shear measurement device, characterized in that the resonance shear measurement device has: a waveform generator; a power supply connected to the waveform generator; a resonance shear measurement unit connected to the power supply and inputted Signal U in ; displacement meter, connected with the resonance shear measurement unit; resonance shear measurement device, connected with the displacement meter and the power supply and input and output signal U out and input signal U in , the resonance shear measurement device There is a timing part, a Fourier transform part connected with the timing part and the displacement meter, an amplitude spectrum generation part connected with the Fourier transform part, a standard part of the amplitude (U out /U in ), and a resonance shear curve made part; and a computer connected to the waveform generator and the resonance shear measuring device.
(10)一种双路型切变应力测定方法,其特征在于,在该双路型切变应力测定方法中将激光光照射到安装在试样的下部表面保持体的底面的反射镜,组合根据来自所述反射镜的反射光的相位变化来对所述试样的表面间距离位移进行测定的双路表面间距离测定方法和根据共振曲线来对所述试样的粘弹性以及摩擦·润滑特性进行测定的测定法,对试样的切变应力进行测定。(10) A two-way type shear stress measurement method, characterized in that, in the two-way type shear stress measurement method, laser light is irradiated to a reflector installed on the bottom surface of the lower surface holder of the sample, and the combination A two-way surface-to-surface distance measurement method that measures the distance displacement between the surfaces of the sample from the phase change of the reflected light from the mirror, and the viscoelasticity, friction and lubrication of the sample from the resonance curve The measurement method for measuring the characteristics is to measure the shear stress of the sample.
(11)一种双路型切变应力测定装置,其特征在于,该双路型切变应力测定装置具有:精密切变装置,使试样的上部表面保持体沿着水平方向位移;位移计,对所述试样的上部表面保持体的向水平方向的位移进行检测;由板簧构成的所述试样的下部表面固定单元,在前端保持所述试样的下部表面保持体且具有在所述下部表面保持体的底面配置的反射镜;驱动装置,驱动该下部表面固定单元来对所述试样的下部表面保持体沿着上下进行驱动;和双路表面间距离测定单元,向所述反射镜照射激光光,根据来自所述反射镜的反射光的相位变化对所述试样的上部表面和所述试样的下部表面间的距离进行测定,其中,对所述试样的上部表面和所述试样的下部表面间的每个距离的所述试样的粘弹性以及摩擦·润滑特性进行测定。(11) A two-way type shear stress measuring device is characterized in that the two-way type shear stress measuring device has: a precision variable device, which makes the upper surface holder of the sample displace along the horizontal direction; , the horizontal displacement of the upper surface holder of the sample is detected; the lower surface fixing unit of the sample composed of a leaf spring holds the lower surface holder of the sample at the front end and has a a reflector arranged on the bottom surface of the lower surface holder; a driving device for driving the lower surface fixing unit to drive the lower surface holder of the sample up and down; and a two-way inter-surface distance measuring unit for the The reflector is irradiated with laser light, and the distance between the upper surface of the sample and the lower surface of the sample is measured according to the phase change of the reflected light from the reflector, wherein the upper surface of the sample is The viscoelasticity and friction/lubricity properties of the sample were measured for each distance between the surface and the lower surface of the sample.
(12)在上述(11)记载的双路型切变应力测定装置中,其特征在于,根据所述试样的共振曲线来对所述试样的粘弹性以及摩擦·润滑特性进行测定。(12) In the two-way shear stress measuring device described in (11) above, the viscoelasticity and friction/lubrication properties of the sample are measured based on the resonance curve of the sample.
(13)在上述(11)或(12)记载的双路型切变应力测定装置中,其特征在于,所述试样为透明试样或不透明试样。(13) In the dual-channel shear stress measuring device described in (11) or (12) above, the sample is a transparent sample or an opaque sample.
(14)在上述(11)或(12)记载的双路型切变应力测定装置中,其特征在于,所述试样为液体薄膜。(14) In the dual-channel shear stress measuring device described in (11) or (12) above, the sample is a liquid thin film.
(15)在上述(11)或(12)记载的双路型切变应力测定装置中,其特征在于,所述试样为液晶薄膜。(15) In the two-way shear stress measuring device described in the above (11) or (12), the sample is a liquid crystal film.
(16)在上述(11)或(12)记载的双路型切变应力测定装置中,其特征在于,所述试样为高分子·表面活性剂等吸附层、化学修饰膜。(16) In the two-way shear stress measuring device described in (11) or (12) above, the sample is an adsorption layer of a polymer, surfactant, or the like, or a chemically modified film.
(17)在上述(11)或(12)记载的双路型切变应力测定装置中,其特征在于,所述试样的上部表面保持体以及下部表面保持体中的一方或两方为不透明基板。(17) In the two-way shear stress measuring device described in the above (11) or (12), one or both of the upper surface holder and the lower surface holder of the sample are opaque. substrate.
附图说明 Description of drawings
图1是表示本发明的实施例的共振切变测定系统的示意图。FIG. 1 is a schematic diagram showing a resonance shear measurement system according to an embodiment of the present invention.
图2是表示本发明的实施例的示出共振切变测定系统的共振切变测定单元的一个例子的示意图。2 is a schematic diagram illustrating an example of a resonance shear measurement unit of a resonance shear measurement system according to an embodiment of the present invention.
图3是表示本发明的变形例的共振切变测定系统的共振切变测定单元的部分结构示意图。3 is a schematic partial configuration diagram showing a resonance shear measurement unit of a resonance shear measurement system according to a modified example of the present invention.
图4是表示本发明的实施例的头振切变测定流程图。Fig. 4 is a flowchart showing head vibration shear measurement according to an embodiment of the present invention.
图5示出在本发明的共振切变测定单元上设置试样并进行测定时的单侧表面的衰减振动例子的图。Fig. 5 is a diagram showing an example of attenuated vibration of one side surface when a sample is set on the resonance shear measurement unit of the present invention and the measurement is performed.
图6是示出针对图5所示的衰减振动进行本发明的傅立叶变换来取得的共振切变曲线和通过以往的方法来取得的各自的曲线的图。6 is a diagram showing a resonance shear curve obtained by performing Fourier transform of the present invention on the damped vibration shown in FIG. 5 and respective curves obtained by a conventional method.
图7是表示本发明的另一实施例的双路型切变应力测定装置的示意图。Fig. 7 is a schematic diagram showing a two-way shear stress measuring device according to another embodiment of the present invention.
图8是表示本发明的另一实施例的为了示出双路型切变应力测定装置的应用例子而使用的试样的示意图。Fig. 8 is a schematic view showing a sample used to illustrate an application example of a two-way shear stress measuring device according to another embodiment of the present invention.
图9是本发明的另一实施例的云母表面中夹入的作为试样的液晶(4-cyano-4-hexyl biphenyl,6CB)的化学式。9 is a chemical formula of liquid crystal (4-cyano-4-hexyl biphenyl, 6CB) as a sample sandwiched in the surface of mica according to another embodiment of the present invention.
图10是表示本发明的另一实施例的示出使用本发明的双路型切变应力测定装置来对作为试样的液晶(4-cyano-4-hexyl biphenyl,6CB)进行测定的结果的图。Fig. 10 shows another example of the present invention and shows the result of measuring liquid crystal (4-cyano-4-hexyl biphenyl, 6CB) as a sample using the two-way shear stress measuring device of the present invention. picture.
具体实施方式 Detailed ways
在本发明的第1共振切变测定方法及其装置中,将输入信号Uin输入到共振切变测定单元的压电(piezo)元件,使用位移计对该共振切变测定单元中的固体表面中夹入的试样的单侧表面的振动进行检测来作为输出信号Uout,与所述输入信号Uin一起,将所述输出信号Uout输入到共振切变计量装置,将所述共振切变测定单元的固体表面中夹入的试样的剪切响应与膜厚的变化一起进行计量,其中,对所述试样的单侧表面的振动的衰减曲线进行傅立叶变换,来取得共振切变曲线。In the first resonance shear measurement method and its device of the present invention, the input signal U in is input to the piezoelectric (piezo) element of the resonance shear measurement unit, and the solid surface in the resonance shear measurement unit is detected using a displacement meter. The vibration of the surface of one side of the sample clamped in is detected as the output signal U out , together with the input signal U in , the output signal U out is input to the resonance shear measurement device, and the resonance shear The shear response of the sample sandwiched in the solid surface of the variable measurement unit is measured together with the change in film thickness, wherein the decay curve of the vibration of the one-sided surface of the sample is Fourier transformed to obtain the resonance shear curve.
本发明的第2双路型切变应力测定装置具有:精密切变装置,使试样的上部表面沿着水平方向位移;位移计,对该试样的上部表面的向水平方向的位移进行检测;由板簧构成的所述试样的下部表面固定单元,在前端保持所述试样的下部表面且具有在其底面配置的反射镜;驱动装置,驱动该下部表面固定单元来对所述试样A的下部表面沿着上下进行驱动;以及双路表面间距离测定单元,根据来自所述反射镜的反射光的相位变化对所述试样A的上部表面和所述试样的下部表面间的距离进行测定,对每个所述试样的上部表面和所述试样的下部表面间的距离的所述试样的粘弹性以及摩擦·润滑特性进行测定。The second two-way type shear stress measuring device of the present invention has: a precision variable device for displacing the upper surface of the sample along the horizontal direction; a displacement meter for detecting the displacement of the upper surface of the sample in the horizontal direction The lower surface fixing unit of the sample composed of a plate spring holds the lower surface of the sample at the front end and has a reflector arranged on its bottom surface; the driving device drives the lower surface fixing unit to adjust the lower surface of the sample. The lower surface of the sample A is driven up and down; and the two-way inter-surface distance measuring unit measures the distance between the upper surface of the sample A and the lower surface of the sample according to the phase change of the reflected light from the mirror. The distance between the upper surface of each sample and the lower surface of the sample was measured, and the viscoelasticity and friction and lubrication characteristics of the sample were measured for each distance between the upper surface of the sample and the lower surface of the sample.
实施例子Implementation example
以下,对本发明的实施方式进行详细说明。Hereinafter, embodiments of the present invention will be described in detail.
图1是表示本发明的实施例的共振切变测定系统的示意图,图2是示出该共振切变测定单元的一个例子的示意图。在该图中,1为波形发生器,2为与波形发生器1连接的电源,3为与电源2连接且输入作为输入信号的输入电压Uin的共振切变测定单元,4为与共振切变测定单元3连接的位移计、例如静电电容位移计,5为与静电电容位移计4以及电源2连接且输入作为输出信号的输出电压Uout以及输入电压Uin的共振切变计量装置,该共振切变计量装置5由计时部5A、傅立叶变换部5B、振幅谱生成部5C、振幅(Uout/Uin)的标准部[以Uin(ω)以及Uout的标准化部]5D、以及共振切变曲线制成部5E构成。6为与共振切变计量装置5连接的个人计算机(PC)6,该个人计算机(PC)6与波形发生器1连接。另外,作为上述的位移计,还可以使用应变仪。FIG. 1 is a schematic diagram showing a resonance shear measurement system according to an embodiment of the present invention, and FIG. 2 is a schematic diagram showing an example of the resonance shear measurement unit. In this figure, 1 is a waveform generator, 2 is a power supply connected to the waveform generator 1, 3 is a resonance shear measurement unit connected to the power supply 2 and inputting an input voltage U in as an input signal, and 4 is a resonance shear measurement unit. The displacement meter connected to the measurement unit 3, such as an electrostatic capacitance displacement meter, 5 is a resonance shear measuring device connected to the electrostatic capacitance displacement meter 4 and the power supply 2 and inputting the output voltage U out and the input voltage U in as the output signal. The resonance shear measuring device 5 is composed of a timing unit 5A, a Fourier transform unit 5B, an amplitude spectrum generation unit 5C, a standard unit [U in (ω) and U out standardization unit] 5D of the amplitude (U out /U in ), and The resonance shear curve forming part 5E is constituted. 6 is a personal computer (PC) 6 connected to the resonance shear measurement device 5 , and the personal computer (PC) 6 is connected to the waveform generator 1 . In addition, a strain gauge may also be used as the displacement gauge described above.
在图2中,10为共振切变测定单元(在图1中与共振切变测定单元3对应),11为悬臂,12为盘支座(disc holder),13为白光,14为固定在盘支座12上的下部基板,15为作为对上部表面沿着水平方向进行驱动的水平驱动部的4分割压电元件,16为固定在该4分割压电元件15的底部的上部基板,17为支撑4分割压电元件15的板簧。18为对板簧17的水平方向位移Δx进行计量的静电电容位移计(探针)(与图1中的静电电容位移计4对应),19为成为剪切响应的测定对象的试样(固体、液体、液晶等)。另外,此处,液体不限于单一成分,还可以是包括2种以上的分子团或胶体分散系的各种溶液。另外,作为上述的水平驱动部,还可以使用电动机。In Fig. 2, 10 is the resonance shear measurement unit (corresponding to the resonance shear measurement unit 3 in Fig. 1), 11 is the cantilever, 12 is the disc holder (disc holder), 13 is the white light, and 14 is fixed on the disc The lower substrate on the
图3是表示本发明的变形例的共振切变测定系统的共振切变测定单元的部分结构示意图。3 is a schematic partial configuration diagram showing a resonance shear measurement unit of a resonance shear measurement system according to a modified example of the present invention.
在该例子中,还可以将基板本身设为试样21、22,不像图2所示那样在基板间夹入试样,就能够对试样(基板)21和试样(基板)22的相互的摩擦(润滑)特性进行测定。In this example, the substrates themselves can also be used as
图4为该共振切变测定流程图。Fig. 4 is a flowchart of the resonance shear measurement.
(1)首先,向压电元件(图2的4分割压电元件15)输入图1所示的振幅电压Uin的正弦波(角频率ω)(步骤S1)。(1) First, the sine wave (angular frequency ω) of the amplitude voltage U in shown in FIG. 1 is input to the piezoelectric element (the quartered
(2)取得输出电压Uout(ω)(步骤S2)。(2) Obtain the output voltage U out (ω) (step S2).
(3)使输入电压Uin停止(步骤S3)。(3) Stop the input voltage U in (step S3).
(4)取得输出电压Uout和经过时间(步骤S4)。(4) Obtain the output voltage U out and the elapsed time (step S4).
(5)进行傅立叶变换(步骤S5)。(5) Perform Fourier transform (step S5).
(6)输出振幅谱(步骤S6)。(6) Output the amplitude spectrum (step S6).
(7)以输出电压Uout(ω)以及输入电压Uin来进行标准化(步骤S7)。(7) Normalize with the output voltage U out (ω) and the input voltage U in (step S7).
(8)输出共振切变曲线(步骤S8)。(8) Outputting the resonance shear curve (step S8).
当在上述的共振切变测定单元上设置试样并进行测定时,试样的单侧表面的衰减振动描绘出图5那样的曲线。When a sample is set on the above-mentioned resonance shear measurement unit and measured, the damped vibration of one surface of the sample draws a curve like that shown in FIG. 5 .
此处,横轴表示经过时间,纵轴表示振动的振幅。在该衰减振动中进行通过以下的式子所表示的傅立叶变换,Here, the horizontal axis represents elapsed time, and the vertical axis represents the amplitude of vibration. In this damped vibration, Fourier transform represented by the following formula is performed,
取得该振幅谱,从而取得共振切变曲线。此处,ω表示角振动数,F(ω)表示所取得的傅立叶谱,f(t)表示衰减振动,t表示时间。This amplitude spectrum is taken to obtain a resonance shear curve. Here, ω represents the number of angular vibrations, F(ω) represents the obtained Fourier spectrum, f(t) represents the damped vibration, and t represents time.
以下,示出针对共振切变曲线通过本发明的共振切变测定方法来测定的结果和通过以往的方法取得的结果。The results obtained by the resonance shear curve of the present invention and the results obtained by the conventional method are shown below.
图6是示出针对图5所示的衰减振动进行本发明的傅立叶变换来取得的共振切变曲线和通过以往的方法来取得的各自的曲线的图。6 is a diagram showing a resonance shear curve obtained by performing Fourier transform of the present invention on the damped vibration shown in FIG. 5 and respective curves obtained by a conventional method.
横轴表示试样的单侧表面的振动数,纵轴表示振动振幅,通过对切变测定单元的压电器附加的输入电压(UIN)和使用静电电容计测定的输出电压(UOUT)之比来表示。以往的方法是一个点一个点地对与各振动频率对应的单侧表面的响应进行测定的方法。图6示出本发明是可更良好地对与频率对应的单侧表面的响应进行测定,且可以以短时间连续地对与宽范围的振动频率对应的试样的单侧表面的响应进行测定的方法。The horizontal axis represents the vibration frequency of one side of the sample, and the vertical axis represents the vibration amplitude. The difference between the input voltage (U IN ) applied to the piezoelectric device of the shear measurement unit and the output voltage (U OUT ) measured by the capacitance meter than to express. The conventional method is to measure the response of one side surface corresponding to each vibration frequency point by point. Figure 6 shows that the present invention can better measure the response of the one-sided surface corresponding to the frequency, and can continuously measure the response of the one-sided surface of the sample corresponding to a wide range of vibration frequencies in a short time Methods.
另外,根据本发明,可将试样(固体、液体、液晶等)夹入2个固体基板间,一边改变其厚度,一边对试样的粘弹性变化、摩擦·润滑特性、试样和固体基板的结合强度等进行评价。另外,还可以将基板本身设为试样,不在其间夹入试样,而能够对相互的摩擦(润滑)特性进行测定。另外,还可以通过吸附或化学修饰法[LB(Langmuir·Brochette)修饰法]等来对该表面进行修饰。另外,不仅仅使单侧表面沿着水平方向振动,还可以使表面沿着垂直方向振动来对试样的频率响应进行测定。In addition, according to the present invention, a sample (solid, liquid, liquid crystal, etc.) can be sandwiched between two solid substrates, and the thickness of the sample can be changed while changing the viscoelasticity of the sample, friction and lubrication characteristics, the sample and the solid substrate. The bonding strength was evaluated. In addition, the substrate itself may be used as a sample, and mutual friction (lubricating) characteristics may be measured without sandwiching the sample therebetween. In addition, the surface can also be modified by adsorption or a chemical modification method [LB (Langmuir·Brochette) modification method] or the like. In addition, the frequency response of the sample can be measured by vibrating the surface not only in the horizontal direction but also in the vertical direction.
根据本发明,无需如以往技术那样按照1个1个点地对各振动频率下的剪切响应进行测定,就可以以短时间简便且准确地对共振切变曲线进行测定。According to the present invention, the resonance shear curve can be measured simply and accurately in a short time without measuring the shear response at each vibration frequency one by one as in the prior art.
接下来,对本发明的另一实施例的双路型切变应力测定进行说明。Next, a two-way type shear stress measurement according to another embodiment of the present invention will be described.
图7是表示本发明的实施例的双路型切变应力测定装置的示意图。Fig. 7 is a schematic diagram showing a two-way shear stress measurement device according to an embodiment of the present invention.
在该图中,31为共振切变测定单元,32为对上部表面沿着水平方向进行驱动的4分割压电元件,33为支撑4分割压电元件32的板簧,34为对板簧33的水平方向位移Δx进行计量的静电电容位移计(探针),35为固定在4分割压电元件32的底部的上部基板。In this figure, 31 is a resonance shear measurement unit, 32 is a four-divided piezoelectric element that drives the upper surface in the horizontal direction, 33 is a leaf spring supporting the four-divided
另外,固定试样A的下部表面保持体42的单元40在板簧41的前端保持试样A的下部表面保持体42,在该下部表面保持体42的下面配置有反射镜43。另一方面,在板簧41的基部具有对该板簧41沿着上下进行驱动的驱动装置[例如,电动机(未图示)]。In addition, the
另外,51为双路表面间距离测定装置,具有:激光光源52;衍射光栅53,接受来自该激光光源52的激光光,并分离成计量光和基准光;压电元件54,对该衍射光栅53进行调整;透镜55,接受来自衍射光栅53的光;固定反射镜56,接受作为该激光光的一部分的基准光;衍射光栅57,再次经由透镜55接受由该固定反射镜56反射的基准光以及由设计在试样A的下部表面保持体52的底面的反射镜43反射的计量光;光电二极管58,接受来自该衍射光栅57的光;以及个人计算机59,与压电元件54和光电二极管58连接。In addition, 51 is a two-way surface-to-surface distance measuring device, which has: a
由于这样构成,使用双路表面间距离测定装置51来对夹入试样A的表面间的距离的变化进行测定,将试样A的上部表面安装到精密切变共振测定单元31上,对试样的粘弹性以及摩擦·润滑特性进行测定,由此,可精密地进行切变应力测定。Due to such a configuration, the change in the distance between the surfaces sandwiching the sample A is measured using the two-way
图8是为了示出本发明的双路型切变应力测定装置的应用例子而使用的试样的示意图,图9是作为该试样的液晶(4-cyano-4-hexyl biphenyl,6CB)的化学式,图10是示出使用本发明的双路型切变应力测定装置来对作为该试样的液晶(4-cyano-4-hexyl biphenyl,6CB)进行测定的共振曲线的图。Fig. 8 is a schematic diagram of a sample used in order to show an application example of the two-way type shear stress measuring device of the present invention, and Fig. 9 is a liquid crystal (4-cyano-4-hexyl biphenyl, 6CB) as the sample Chemical formula, FIG. 10 is a graph showing the resonance curve measured for the liquid crystal (4-cyano-4-hexyl biphenyl, 6CB) as the sample using the two-way shear stress measuring device of the present invention.
如图8所示,在作为试样的液晶(4-cyano-4-hexyl biphenyl,6CB)61的上下配置云母62、63。即,配置成在作为上部基板35的云母62和作为下部表面保持体42的云母63之间夹入作为试样的液晶61。As shown in FIG. 8 , mica 62 and 63 are arranged above and below a liquid crystal (4-cyano-4-hexyl biphenyl, 6CB) 61 as a sample. That is, it is arranged so that liquid crystal 61 as a sample is sandwiched between mica 62 as
该云母表面中夹入的作为试样的液晶(4-cyano-4-hexyl biphenyl,6CB)的化学式如图9所示。The chemical formula of the sample liquid crystal (4-cyano-4-hexyl biphenyl, 6CB) sandwiched in the mica surface is shown in FIG. 9 .
在图10中,横轴表示试样上部的表面的角振动数(s-1),纵轴表示针对精度切变共振测定单元的压电元件的输入电压(Uin)和由静电电容位移计测定的输出电压(Uout)之比。除了对作为试样的液晶进行测定得出的结果以外,为了对以不夹入作为试样的液晶而离开保持体的表面的状态测定的结果[空气中(分离侧)]、和使保持体的表面接触来测定的结果[空气中(云母-云母接触)]进行比较而进行描绘。试样的表面间距离的横实线表示该距离下的共振峰值。此处,对于表面间距离,当使用驱动装置来对下部表面保持体向上方进行驱动时,将表面间距离没有变化的点定义为0nm。随着表面间距离变化,观察到共振曲线的变化。存在多个0nm的峰值的现象表示表面距离恒定且负荷发生变化的情况。In FIG. 10, the horizontal axis represents the angular vibration number (s -1 ) of the upper surface of the sample, and the vertical axis represents the input voltage (U in ) to the piezoelectric element of the precision shear resonance measurement unit and the voltage measured by the capacitance displacement meter. The measured output voltage (U out ) ratio. In addition to the results obtained by measuring the liquid crystal as a sample, for the results measured in a state where the liquid crystal as a sample is not sandwiched and separated from the surface of the holder [in the air (separation side)], and the holder The results of surface contact measurements [in air (mica-mica contact)] are compared and plotted. The horizontal solid line of the distance between the surfaces of the sample indicates the resonance peak at the distance. Here, regarding the distance between surfaces, when the lower surface holder is driven upward using a driving device, the point at which the distance between surfaces does not change is defined as 0 nm. As the distance between the surfaces varies, a change in the resonance curve is observed. The phenomenon that there are many peaks of 0 nm indicates that the surface distance is constant and the load varies.
另外,根据本发明,可将试样(液体、固体、液晶等)夹入2个固体基板间,一边使其厚度改变,一边对试样的粘弹性变化、摩擦·润滑特性、试样和固体基板的结合强度等进行评价。另外,还可以将基板本身设为试样,不在基板间夹入试样,而对相互的摩擦(润滑)特性进行测定。另外,还可以通过吸附或化学修饰法[LB(Langmuir·Brochette法)]等来对该表面进行修饰。In addition, according to the present invention, a sample (liquid, solid, liquid crystal, etc.) can be sandwiched between two solid substrates, and the thickness of the sample can be changed while changing the viscoelasticity of the sample, friction and lubrication characteristics, and the difference between the sample and the solid. The bonding strength of the substrate and the like were evaluated. In addition, the substrate itself may be used as a sample, and the mutual friction (lubricating) characteristics may be measured without sandwiching the sample between the substrates. In addition, the surface can also be modified by adsorption or a chemical modification method [LB (Langmuir·Brochette method)] or the like.
另外,由于使用激光的反射光,所以无需使光透过基板以及试样,即使在使用不透明基板以及不透明试样的情况下,也可以对表面间距离进行测定,在各距离下对试样的粘弹性以及摩擦·润滑特性进行测定。In addition, since the reflected light of the laser light is used, it is not necessary to transmit light through the substrate and the sample, and the distance between surfaces can be measured even when an opaque substrate and opaque sample are used. Viscoelasticity and friction and lubrication properties were measured.
另外,本发明不限于上述实施例,可根据本发明的宗旨进行各种变形,不将这些从本发明的范围排出。In addition, the present invention is not limited to the above-mentioned embodiments, and various modifications can be made according to the gist of the present invention, and these are not excluded from the scope of the present invention.
产业上的可利用性Industrial availability
本发明的第1共振切变测定方法特别适用于固体表面间的具有纳米等级的厚度的液体薄膜的物性的简便且准确的计量。The first resonance shear measurement method of the present invention is particularly suitable for the simple and accurate measurement of the physical properties of a liquid thin film having a nanometer-order thickness between solid surfaces.
本发明的第2双路型切变应力测定装置可利用为可使用用于对不透明基板间的距离进行测定的双路法来进行精密的切变应力测定的双路型切变应力测定装置,与第1共振切变测定方法同样地,适用于固体表面间的具有纳米等级的厚度的液体薄膜的物性的简便且准确的计量。The second two-way type shear stress measuring device of the present invention can be utilized as a two-way type shear stress measuring device capable of precise shear stress measurement using a two-way method for measuring the distance between opaque substrates, Similar to the first resonance shear measurement method, it is suitable for the simple and accurate measurement of the physical properties of a liquid thin film having a nanometer-order thickness between solid surfaces.
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CN102221499B (en) * | 2011-03-29 | 2012-10-03 | 天津大学 | Alignment loading device used for stretching test of nanoscale, micron-size thin film materials |
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